CN103447015A - Desorption and regeneration method for organic matter adsorbent - Google Patents
Desorption and regeneration method for organic matter adsorbent Download PDFInfo
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Description
（一）技术领域(1) Technical field
本发明涉及一种有机污染物吸附剂的再生方法，尤其针对有机分子在活性炭、分子筛和高分子树脂吸附剂内的再生脱附，解决目前有机废气、有机废水吸附后吸附剂再生的问题。The invention relates to a regeneration method of an organic pollutant adsorbent, especially aimed at the regeneration and desorption of organic molecules in activated carbon, molecular sieves and polymer resin adsorbents, and solves the current problem of adsorbent regeneration after adsorption of organic waste gas and organic waste water.
（二）背景技术(2) Background technology
吸附技术目前被广泛应用在有机废气和有机废水治理中，尤其是针对一些低浓度的有机废气和废水，吸附可以很好地去除有机污染物，达到净化的目的。另外，通过脱附回收利用，也可以实现有机污染物的资源化利用。目前工业上最常见的吸附剂有活性炭、活性炭纤维、沸石分子筛和高分子多孔树脂等，这些吸附剂都表现出良好的吸附特性。但在有机污染处理中，除了要求吸附剂具有高效吸附性能外，同样要求吸附剂可以良好的再生性能，因此脱附也是有机污染物净化的关键技术。目前研究较多的脱附技术有：溶剂洗脱、热空气脱附和水蒸气脱附技术等，但溶剂洗脱和热空气脱附易造成后续处理的二次污染，而且有机物无法实现资源利用。因此在有机物脱附回收中，得到最为广泛应用的是水蒸气脱附技术。通过大量高温水蒸气传热，使吸附有机分子受热脱附，在后续冷凝中和水蒸气一起转化为液体，从而实现有机物的回收。Adsorption technology is currently widely used in the treatment of organic waste gas and organic wastewater, especially for some low-concentration organic waste gas and wastewater. Adsorption can remove organic pollutants well and achieve the purpose of purification. In addition, through desorption and recycling, the resource utilization of organic pollutants can also be realized. At present, the most common adsorbents in the industry include activated carbon, activated carbon fiber, zeolite molecular sieve and polymer porous resin, etc., and these adsorbents all show good adsorption characteristics. However, in the treatment of organic pollution, in addition to the high-efficiency adsorption performance of the adsorbent, it is also required that the adsorbent can have good regeneration performance, so desorption is also a key technology for the purification of organic pollutants. At present, there are many desorption technologies studied: solvent elution, hot air desorption and water vapor desorption, etc., but solvent elution and hot air desorption are easy to cause secondary pollution in subsequent treatment, and organic matter cannot be used as a resource. Therefore, in the desorption and recovery of organic matter, the most widely used is the water vapor desorption technology. Through the heat transfer of a large amount of high-temperature water vapor, the adsorbed organic molecules are desorbed by heat, and converted into liquid together with water vapor in the subsequent condensation, so as to realize the recovery of organic matter.
但在工业实践中，水蒸气再生技术同样存在几个问题：（1）利用水蒸气温度加热吸附剂，要消耗大量水蒸气；（2）水蒸气热量从外传递到吸附剂孔道内，而分子筛和树脂等吸附剂热导系数小，热传递速率慢，脱附时间长；（3）水分子会在吸附剂内残留，吸附剂需热空气进行干燥，能耗较高；（4）脱附产物含水率高，给后续储存和分离带来困难。However, in industrial practice, water vapor regeneration technology also has several problems: (1) using the water vapor temperature to heat the adsorbent consumes a large amount of water vapor; Adsorbents such as resin and resin have small thermal conductivity, slow heat transfer rate, and long desorption time; (3) water molecules will remain in the adsorbent, and the adsorbent needs hot air to dry, which consumes a lot of energy; (4) desorption The high water content of the product brings difficulties to subsequent storage and separation.
为进一步提高脱附速率，微波再生技术成为近年来的研究热点，通过微波作用，可使活性炭迅速升温，从而使吸附在表面的有机分子快速脱附，大大减少脱附时间，并且通过后续冷凝，得到较为单一的有机液体产物。但微波处理同样也存在一些局限性：（1）首先微波处理活性炭等高介电常数的介质，容易产生局部高温和火花，存在严重的安全隐患，并且会破坏吸附剂结构；（2）相对于高疏水性的吸附剂（如树脂、高疏水性的沸石分子筛）和非极性的吸附质（苯、甲苯），由于介电常数低，微波几乎不能加热这些介质，因此也不能达到良好的脱附效果。In order to further increase the desorption rate, microwave regeneration technology has become a research hotspot in recent years. Through microwave action, the temperature of activated carbon can be raised rapidly, so that the organic molecules adsorbed on the surface can be desorbed quickly, greatly reducing the desorption time, and through subsequent condensation, A relatively simple organic liquid product is obtained. However, microwave treatment also has some limitations: (1) Firstly, microwave treatment of media with high dielectric constant such as activated carbon is prone to local high temperature and sparks, which has serious safety hazards and will destroy the structure of the adsorbent; (2) Compared with Highly hydrophobic adsorbents (such as resins, highly hydrophobic zeolite molecular sieves) and non-polar adsorbates (benzene, toluene), due to the low dielectric constant, microwaves can hardly heat these media, so good desorption can not be achieved. With effect.
因此迫切需要一种新的脱附再生技术，不仅使用安全高效，而且能适应不同极性的吸附剂和吸附质，回收得到低含水率的有机物。Therefore, there is an urgent need for a new desorption regeneration technology, which is not only safe and efficient, but also adaptable to adsorbents and adsorbates of different polarities, and recovers organic matter with low water content.
（三）发明内容(3) Contents of the invention
本发明的目的是提供一种新的吸附剂表面有机物脱附技术，可提高脱附速率，降低能耗，以及减小有机物和水的分离的负荷。The purpose of the present invention is to provide a new adsorbent surface organic matter desorption technology, which can increase the desorption rate, reduce energy consumption, and reduce the separation load of organic matter and water.
为实现上述目的，本发明采用的技术方案是：In order to achieve the above object, the technical scheme adopted in the present invention is:
一种有机物吸附剂的脱附再生方法，所述方法为：在脱附塔内设有微波发生器的有机物吸附剂的脱附再生装置内，将待脱附的吸附有有机物的吸附剂置于脱附塔内，从脱附塔顶端蒸气入口通入水蒸气，开启微波发生器，微波功率500-10000W，进行脱附处理2～30分钟，脱附的有机物和水蒸气从脱附塔底端蒸气出口流出，进入冷凝器冷凝；然后切断水蒸气，从脱附塔顶端氮气入口通入氮气，底端氮气出口流出氮气，微波功率为200-2000W，进行干燥处理2-20分钟，停止微波发生器并切断氮气，即得到脱附后的吸附剂。A method for desorption and regeneration of an organic matter adsorbent, the method comprising: in a desorption regeneration device for an organic matter adsorbent provided with a microwave generator in a desorption tower, the adsorbent to be desorbed and adsorbed with organic matter is placed in the In the desorption tower, water vapor is introduced from the steam inlet at the top of the desorption tower, the microwave generator is turned on, the microwave power is 500-10000W, and the desorption treatment is carried out for 2 to 30 minutes. The desorbed organic matter and water vapor are steamed from the bottom of the desorption tower. The outlet flows out and enters the condenser to condense; then cut off the water vapor, feed nitrogen gas from the nitrogen inlet at the top of the desorption tower, and nitrogen gas flows out from the nitrogen outlet at the bottom of the desorption tower. The microwave power is 200-2000W, carry out drying treatment for 2-20 minutes, and stop the microwave generator And cut off the nitrogen to obtain the desorbed adsorbent.
所述微波功率可根据吸附塔内体积大小进行调节，使微波场均匀作用整个吸附塔。The microwave power can be adjusted according to the volume inside the adsorption tower, so that the microwave field acts uniformly on the entire adsorption tower.
所述水蒸气每小时通入的体积量为吸附剂体积的0.2-5.0倍，其用量根据吸附剂介电常数不同而进行适当调节。The volume of the water vapor introduced per hour is 0.2-5.0 times the volume of the adsorbent, and the amount used is properly adjusted according to the different dielectric constants of the adsorbent.
所述氮气的空速为500-5000h-1，优选为2000h-1。The space velocity of the nitrogen is 500-5000h -1 , preferably 2000h -1 .
本发明还提供一种有机物吸附剂的脱附再生装置，所述装置包括脱附塔、蒸气发生器、氮气发生器、冷凝器，以及设于脱附塔内的微波发生器，所述蒸气发生器通过流量计与脱附塔顶端的蒸气入口连通，氮气发生器通过流量计与脱附塔顶端的氮气入口相连通，氮气出口和蒸气出口分别设于脱附塔底端，蒸气出口与冷凝器连通。The present invention also provides a desorption and regeneration device for organic matter adsorbent, said device comprises a desorption tower, a steam generator, a nitrogen generator, a condenser, and a microwave generator arranged in the desorption tower, said steam generator The device is connected with the steam inlet at the top of the desorption tower through a flow meter, the nitrogen generator is connected with the nitrogen inlet at the top of the desorption tower through a flow meter, the nitrogen outlet and the steam outlet are respectively arranged at the bottom of the desorption tower, and the steam outlet is connected with the condenser. connected.
脱附塔内可填装待脱附的吸附剂，所述吸附剂可以为活性炭、活性炭纤维、沸石分子筛、高分子多孔树脂等各种可吸附有机物的吸附剂。蒸气发生器通过流量计调节水蒸气流量，氮气发生器通过流量计调节氮气流量。The adsorbent to be desorbed can be filled in the desorption tower, and the adsorbent can be activated carbon, activated carbon fiber, zeolite molecular sieve, polymer porous resin and other adsorbents capable of adsorbing organic matter. The steam generator adjusts the water vapor flow through the flow meter, and the nitrogen generator adjusts the nitrogen flow through the flow meter.
所述装置可于冷凝器出口连接一存储容器，存储从冷凝器中冷凝出来的液态的有机物和水。The device can be connected with a storage container at the outlet of the condenser to store liquid organic matter and water condensed from the condenser.
本发明脱附技术的工作原理如下：蒸汽发生器产生一定量的水蒸汽，水蒸气通入到脱附塔，开启脱附塔内部的微波发生器，使微波场均匀作于整个脱附塔，水蒸气在微波作用下，既防止了水蒸气冷凝，又可进一步被加热升温，热量可迅速传递给有机吸附质，使有机吸附质在孔道内快速脱附，随水蒸气从吸附剂表面脱附出来。另外对于高介电常数的吸附剂，可以快速加热吸附剂，使其表面有机分子脱附。脱附的有机物和水蒸气从脱附塔流出后，经过冷凝器转化为液体，得到的液体进入存储容器，以备后续分离处理。当脱附塔内吸附剂吸附的有机物被脱附完全后，切断水蒸气量，通入氮气，在微波作用下吸附剂内残存的水分子在氮气带动下，脱附出吸附塔放空，从而使吸附剂得到干燥。脱附完全的吸附剂可以回收利用于有机废气或有机废水的吸附。The working principle of the desorption technology of the present invention is as follows: the steam generator generates a certain amount of water vapor, and the water vapor is passed into the desorption tower, and the microwave generator inside the desorption tower is turned on, so that the microwave field is evenly applied to the whole desorption tower, Under the action of microwave, the water vapor not only prevents the water vapor from condensing, but also can be further heated up. The heat can be quickly transferred to the organic adsorbate, so that the organic adsorbate can be desorbed quickly in the pores, and desorbed from the surface of the adsorbent along with the water vapor. come out. In addition, for the adsorbent with high dielectric constant, the adsorbent can be heated rapidly to desorb the organic molecules on its surface. After the desorbed organic matter and water vapor flow out of the desorption tower, they are converted into liquid through the condenser, and the obtained liquid enters the storage container for subsequent separation treatment. When the organic matter adsorbed by the adsorbent in the desorption tower is completely desorbed, the amount of water vapor is cut off, and nitrogen gas is introduced. Under the action of microwaves, the remaining water molecules in the adsorbent are driven by nitrogen and desorbed out of the adsorption tower to be emptied, so that The sorbent is dried. The completely desorbed adsorbent can be recycled for the adsorption of organic waste gas or organic wastewater.
操作过程中，可根据吸附质和吸附剂的介电常数，调节水蒸气的量，如果采用吸附剂为低介电常数的高分子树脂和高疏水性的分子筛，则适当调高水蒸气流量；如果采用的吸附剂为高介电常数的活性炭或活性炭纤维，可以大幅减少通入的水蒸气量。另外，吸附质的极性大小也影响水蒸气通入量。如果脱附的有机物为非极性，可适当增加水蒸汽量；如果脱附的有机物为强极性，可适当降低水蒸气量。本领域技术人员根据实际情况可自行调节。During the operation, the amount of water vapor can be adjusted according to the dielectric constant of the adsorbate and the adsorbent. If the adsorbent is a polymer resin with a low dielectric constant and a molecular sieve with high hydrophobicity, the water vapor flow rate should be increased appropriately; If the adsorbent used is activated carbon or activated carbon fiber with high dielectric constant, the amount of water vapor introduced can be greatly reduced. In addition, the polarity of the adsorbate also affects the water vapor flux. If the desorbed organic matter is non-polar, the amount of water vapor can be appropriately increased; if the desorbed organic matter is strongly polar, the amount of water vapor can be appropriately reduced. Those skilled in the art can adjust by themselves according to the actual situation.
本发明提出的脱附技术的有点在于：（1）通过微波强化水蒸气，使水蒸气保持高温蒸汽状态，可大幅降低水蒸气的用量，降低后续有机物和水的分离负荷，具有节能减排的意义；（2）水蒸汽进入吸附剂孔道内后，在微波作用下可迅速把热量传递给吸附的有机分子，大幅提高有机分子的脱附速率；（3）水蒸气引入，可减少活性炭类吸附剂在微波作用下的局部高温热点和火花，保护吸附剂结构，提高装置的安全性；（4）在微波作用和氮气吹扫下，可实现吸附剂快速的干燥，省略了单一水蒸气脱附中热空气干燥和冷气降温的单元操作，降低了能耗。（5）此套技术适合具有各类不同介电常数吸附剂和极性吸附质的脱附，具有广泛的通用性；The advantages of the desorption technology proposed by the present invention are: (1) microwaves are used to strengthen water vapor to keep the water vapor in a high-temperature steam state, which can greatly reduce the amount of water vapor used, reduce the subsequent separation load of organic matter and water, and have the advantages of energy saving and emission reduction Significance; (2) After water vapor enters the pores of the adsorbent, it can quickly transfer heat to the adsorbed organic molecules under the action of microwaves, greatly increasing the desorption rate of organic molecules; (3) The introduction of water vapor can reduce the adsorption of activated carbon. The local high-temperature hot spots and sparks of the agent under the action of microwave protect the structure of the adsorbent and improve the safety of the device; (4) under the action of microwave and nitrogen purge, the adsorbent can be dried quickly, omitting the single water vapor desorption process. The unit operation of hot air drying and cold air cooling reduces energy consumption. (5) This set of technology is suitable for the desorption of adsorbents with different dielectric constants and polar adsorbates, and has wide versatility;
（四）附图说明(4) Description of drawings
图1：本发明水汽协同微波脱附装置示意图。Figure 1: Schematic diagram of the water vapor synergistic microwave desorption device of the present invention.
图1中，1—水蒸气发生器；2—冷凝器；3—冷凝液体储存容器；4—保温套；5—微波发生器；6—脱附塔；7—氮气发生器。In Fig. 1, 1—steam generator; 2—condenser; 3—condensed liquid storage container; 4—insulation jacket; 5—microwave generator; 6—desorption tower; 7—nitrogen generator.
图2：实施例1中活性炭纤维表面甲苯在不同脱附方法下甲苯残留率的对比图。Figure 2: Comparison chart of toluene residual rate on the surface of activated carbon fiber in Example 1 under different desorption methods.
图3：实施例2中Y型分子筛表面甲苯在不同脱附方法下甲苯残留率的对比图。Figure 3: Comparison chart of toluene residual rate on the surface of Y-type molecular sieve in Example 2 under different desorption methods.
图4：实施例3中多孔高分子树脂聚二乙烯苯（PDVB）表面甲苯在不同脱附方法下甲苯残留率的对比图。Figure 4: A comparison chart of toluene residual rate on the surface of the porous polymer resin polydivinylbenzene (PDVB) in Example 3 under different desorption methods.
（五）具体实施方式(5) Specific implementation methods
下面以具体实施例来对本发明作进一步说明，但本发明的保护范围不限于此。The present invention will be further described below with specific examples, but the protection scope of the present invention is not limited thereto.
实施例1：Example 1:
取活性炭纤维2克，吸附甲苯2克，装入脱附塔，如图1方式搭建脱附装置。脱附塔6内设有微波发生器5，蒸气发生器1通过流量计与脱附塔6顶端的蒸气入口连通，氮气发生器7通过流量计与脱附塔6顶端的氮气入口相连通，氮气出口和蒸气出口分别设于脱附塔6底端，蒸气出口与冷凝器2连通，冷凝器2出口连接一存储容器3，存储从冷凝器中冷凝出来的液态的有机物和水。蒸气发生器1与脱附塔6顶端的蒸气入口之间的管道外设有保温套4，防止蒸气冷凝。Take 2 grams of activated carbon fiber, adsorb 2 grams of toluene, and put it into the desorption tower, and build the desorption device as shown in Figure 1. The
通过以下三种方法进行脱附：Desorption is performed by the following three methods:
（1）微波＋水蒸气：从脱附塔顶端蒸气入口通入水蒸气，水蒸气流量1.0g/min，开启微波发生器，微波功率为600W，进行脱附处理，脱附的有机物和水蒸气从脱附塔底端蒸气出口流出，进入冷凝器冷凝，跟踪监测甲苯残留率，至脱附完全；然后切断水蒸气，从脱附塔顶端氮气入口通入氮气，底端氮气出口流出氮气，氮气空速2000h-1，微波功率为600W，进行干燥处理3分钟，停止微波发生器并切断氮气，即得到脱附后的吸附剂；；(1) Microwave + water vapor: Water vapor is introduced from the steam inlet at the top of the desorption tower, the water vapor flow rate is 1.0g/min, the microwave generator is turned on, the microwave power is 600W, and the desorption process is carried out. The desorbed organic matter and water vapor are removed from the The steam outlet at the bottom of the desorption tower flows out, enters the condenser to condense, and tracks and monitors the residual rate of toluene until the desorption is complete; then cut off the water vapor, feed nitrogen from the nitrogen inlet at the top of the desorption tower, nitrogen flows out of the nitrogen outlet at the bottom, and nitrogen air Speed 2000h -1 , microwave power 600W, carry out drying treatment for 3 minutes, stop the microwave generator and cut off the nitrogen, and obtain the adsorbent after desorption;
（2）微波＋氮气：从脱附塔顶端氮气入口通入氮气，底端氮气出口流出氮气，氮气空速2000h-1，微波功率为600W，跟踪监测甲苯残留率，至脱附完全；(2) Microwave + nitrogen: Nitrogen is introduced from the nitrogen inlet at the top of the desorption tower, and nitrogen flows out from the nitrogen outlet at the bottom. The nitrogen space velocity is 2000h -1 , and the microwave power is 600W. Track and monitor the residual rate of toluene until the desorption is complete;
（3）水蒸气，从脱附塔顶端蒸气入口通入水蒸气，水蒸气流量1.0g/min，进行脱附处理，脱附的有机物和水蒸气从脱附塔底端蒸气出口流出，进入冷凝器冷凝，跟踪监测甲苯残留率，至脱附完全；。(3) Water vapor, water vapor is introduced from the steam inlet at the top of the desorption tower, and the water vapor flow rate is 1.0g/min for desorption treatment. The desorbed organic matter and water vapor flow out from the steam outlet at the bottom of the desorption tower and enter the condenser Condensate, track and monitor the residual rate of toluene until the desorption is complete;
以上三种方式脱附速率对比结果见图2，结果表明，在微波作用下，活性炭纤维表面甲苯可以2分钟之内脱附完全，水蒸气和微波协同作用下比单一微波，脱附速率更快。但采用单一水蒸气脱附，需要近30分钟才能脱附较完全。因此，对于介电常数较大的活性炭纤维吸附剂，微波可以明显提高了脱附速率，水汽协同微波可以进一步加快脱附速率，并且吸附残留物很少。The desorption rate comparison results of the above three methods are shown in Figure 2. The results show that under the action of microwaves, toluene on the surface of activated carbon fibers can be completely desorbed within 2 minutes, and the desorption rate is faster under the synergistic action of water vapor and microwave than single microwave . However, it takes nearly 30 minutes to desorb completely by using a single water vapor desorption. Therefore, for the activated carbon fiber adsorbent with a large dielectric constant, microwave can significantly increase the desorption rate, and water vapor combined with microwave can further accelerate the desorption rate, and the adsorption residue is very little.
实施例2：Example 2:
取Y型分子筛2克，吸附甲苯2克，装入微波脱附塔，按照实施例1的三种方法进行脱附：（1）微波＋水蒸气，微波功率为600W，水蒸气流量1.0g/min；（3）微波＋氮气，氮气空速2000h-1；（2）水蒸气，水蒸气流量1.0g/min。Take 2 grams of Y-type molecular sieves, absorb 2 grams of toluene, put them into a microwave desorption tower, and perform desorption according to the three methods of Example 1: (1) Microwave + water vapor, microwave power is 600W, water vapor flow rate is 1.0g/ min; (3) microwave + nitrogen, nitrogen air velocity 2000h -1 ; (2) water vapor, water vapor flow rate 1.0g/min.
以上三种方式脱附速率对比结果见图3，结果表明，在微波作用下，Y分子筛表面甲苯可以10分钟之内脱附完全。而水蒸气和微波协同作用下比单一微波，脱附速率更快，可在7分钟之内就脱附完全。但采用单一水蒸气脱附，需要近30分钟才能脱附较完全。因此，对于有一定极性的Y分子筛吸附剂，微波可以明显提高脱附速率，水汽协同微波技术可以进一步加快脱附速率，并且吸附残留物很少。The comparison results of the desorption rates of the above three methods are shown in Figure 3. The results show that under the action of microwaves, the toluene on the surface of the Y molecular sieve can be completely desorbed within 10 minutes. Under the synergistic effect of water vapor and microwave, the desorption rate is faster than single microwave, and the desorption can be completed within 7 minutes. However, it takes nearly 30 minutes to desorb completely by using a single water vapor desorption. Therefore, for Y molecular sieve adsorbents with a certain polarity, microwave can significantly increase the desorption rate, and water vapor synergistic microwave technology can further accelerate the desorption rate, and the adsorption residue is very little.
实施例3：Example 3:
取多孔高分子树脂聚二乙烯苯（PDVB）2克，吸附甲苯10克，装入微波脱附塔，按照实施例1的三种方法进行脱附：（1）微波＋水蒸气，微波功率为600W，水蒸气流量1.0g/min；（3）微波＋氮气，氮气空速2000h-1；（2）水蒸气，水蒸气流量1.0g/min。Take 2 grams of porous polymer resin polydivinylbenzene (PDVB), absorb 10 grams of toluene, put it into a microwave desorption tower, and perform desorption according to the three methods of Example 1: (1) microwave+water vapor, microwave power is 600W, water vapor flow rate 1.0g/min; (3) microwave + nitrogen, nitrogen air velocity 2000h -1 ; (2) water vapor, water vapor flow rate 1.0g/min.
以上三种方式脱附速率对比结果见图4，发现，在单一微波作用下，树脂表面甲苯脱附速率很慢，30分钟后，脱附率只达到40％。而水蒸气和微波协同作用下比单一微波，脱附速率大幅提高，可在5分钟之内就脱附完全。但采用单一水蒸气脱附，需要近30分钟才能脱附较完全。因此，对于非极性和低介电常数的高分子树脂吸附剂，单一的微波没有脱附效果，但水汽协同微波技术可大幅提高脱附速率，并且吸附残留物很少。The desorption rate comparison results of the above three methods are shown in Figure 4. It was found that under the action of a single microwave, the toluene desorption rate on the resin surface was very slow, and after 30 minutes, the desorption rate only reached 40%. However, under the synergistic effect of water vapor and microwave, the desorption rate is greatly improved compared with single microwave, and the desorption can be completed within 5 minutes. However, it takes nearly 30 minutes to desorb completely by using a single water vapor desorption. Therefore, for nonpolar and low dielectric constant polymer resin adsorbents, a single microwave has no desorption effect, but water vapor synergistic microwave technology can greatly increase the desorption rate, and the adsorption residue is very small.
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